反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([C:11]1[N:16]=[C:15]([C:17]3[C:18]([N:37]([CH3:42])[S:38]([CH3:41])(=[O:40])=[O:39])=[CH:19][C:20]4[O:24][C:23]([C:25]5[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=5)=[C:22]([C:32]([NH:34][CH3:35])=[O:33])[C:21]=4[CH:36]=3)[CH:14]=[CH:13][C:12]=1[CH2:43][CH2:44][CH2:45]O)[NH:6]2.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>C1COCC1>[F:1][C:2]1[C:3]2[CH:4]=[C:5]3[C:11]4[N:16]=[C:15]([C:17]5[C:18]([N:37]([CH3:42])[S:38]([CH3:41])(=[O:39])=[O:40])=[CH:19][C:20]6[O:24][C:23]([C:25]7[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=7)=[C:22]([C:32]([NH:34][CH3:35])=[O:33])[C:21]=6[CH:36]=5)[CH:14]=[CH:13][C:12]=4[CH2:43][CH2:44][CH2:45][N:6]3[C:7]=2[CH:8]=[CH:9][CH:10]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 5-(6-(4-fluoro-1H-indol-2-yl)-5-(3-hydroxypropyl)pyridin-2-yl)-2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)benzofuran-3-carboxamide (153 mg, 0.237 mmol) and triphenylphosphine (62.2 mg, 0.237 mmol) in THF was added diisopropyl azodicarboxylate (0.046 mL, 0.237 mmol). The resultant mixture was stirred at ambient temperature for 10 h then was concentrated in vacuo and the residue purified by silica gel column chromatography using a step gradient of 0-50-100% EtOAc/Hexanes as eluent. 1H NMR δ (ppm) (CHCl3-d): 8.07 (1H, s), 8.02 (2H, dd, J=8.61, 5.32 Hz), 7.75 (1H, d, J=7.78 Hz), 7.70 (1H, s), 7.60 (1H, d, J=7.77 Hz), 7.26˜7.0 (4H, m), 7.09 (1H, s), 6.85˜6.81 (1H, m), 5.98 (1H, br s), 4.23 (2H, t, J=6.66 Hz), 3.35 (3H, s), 3.03 (3H, d, J=4.90 Hz), 2.85 (2H, t, J=7.00 Hz), 2.80 (3H, s), 2.47˜2.42 (2H, m), MS (M+H)+: 627.
後処理
- concentrationthen was concentrated in vacuo
- customthe residue purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-e3fb3e3b5efb42868e1d52b44f02c8d4
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09243002B2
関連ノート
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